CN114014265A - Liquid organic hydrogen storage device and method - Google Patents
Liquid organic hydrogen storage device and method Download PDFInfo
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- CN114014265A CN114014265A CN202111462269.8A CN202111462269A CN114014265A CN 114014265 A CN114014265 A CN 114014265A CN 202111462269 A CN202111462269 A CN 202111462269A CN 114014265 A CN114014265 A CN 114014265A
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/0005—Reversible uptake of hydrogen by an appropriate medium, i.e. based on physical or chemical sorption phenomena or on reversible chemical reactions, e.g. for hydrogen storage purposes ; Reversible gettering of hydrogen; Reversible uptake of hydrogen by electrodes
- C01B3/001—Reversible uptake of hydrogen by an appropriate medium, i.e. based on physical or chemical sorption phenomena or on reversible chemical reactions, e.g. for hydrogen storage purposes ; Reversible gettering of hydrogen; Reversible uptake of hydrogen by electrodes characterised by the uptaking medium; Treatment thereof
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
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Abstract
The invention discloses a liquid organic hydrogen storage device, which comprises: a feed system for introducing gas and hydrogen storage material; the reaction system comprises an intermittent feeding reaction device, a hydrogen storage material hydrogenation device and a hydrogen storage material hydrogenation device, wherein the intermittent feeding reaction device is used for hydrogenating the hydrogen storage material to react; and the separation system is used for separating and collecting the hydrogenated hydrogen storage material and the redundant hydrogen. The device disclosed by the invention adopts the electromagnetic valve to control the hydrogen storage material to perform intermittent feeding on the trickle bed, so that the contact area of the material and the catalyst is increased, and the reaction efficiency is improved.
Description
Technical Field
The invention relates to the technical field of hydrogen storage, in particular to a liquid organic hydrogen storage system and an intermittent feeding reaction device.
Background
Hydrogen is widely used in large-scale industry in the fields of refining mineral oils, manufacturing materials (e.g. steel, plastics, synthetic resins), bulk chemicals (e.g. ammonia, methanol) and fine chemicals. Most of the hydrogen required for these industrial processes needs to be at least 99.9% pure. Hydrogen is one of the most efficient energy carriers and provides a stable source of power for energy conversion. The safe and efficient utilization of hydrogen energy provides a means to meet the pressing challenges of global greenhouse gases. At the heart of the potential large-scale application of hydrogen technology in the marketplace is the development of large-scale, high-density, and safe storage and transportation of hydrogen, which remains one of the great challenges for today's technology.
In recent years, Liquid Organic Hydrogen Carriers (LOHC) have been developed to store hydrogen, and the LOHC system consists of at least one hydrogen-lean compound and one hydrogen-rich compound. Hydrogen is stored by catalytic reaction with hydrogen-lean compounds of the LOHC system at high hydrogen pressures. The resulting hydrogen-rich LOHC molecules release hydrogen by catalytic dehydrogenation at low hydrogen pressure. Storage of hydrogen in liquid form has incomparable advantages over existing methods of hydrogen storage and transportation.
In the field of hydrogen storage, the currently adopted hydrogen storage method is a traditional chemical reaction kettle or reaction system, and patent number CN105129728A introduces a method for storing hydrogen by using a reaction kettle, wherein the method is carried out in the reaction kettle, and the reaction amount is limited by the volume of the reaction kettle; patent No. CN109027683A describes a hydrogen storage system and control method, which uses a catalytic bed to perform catalytic hydrogenation.
Patent No. CN105129728A describes a method for storing hydrogen by using a reaction kettle, the method is carried out in the reaction kettle, the reaction amount is limited by the volume of the reaction kettle, and the method is only suitable for laboratory experiments and cannot carry out continuous hydrogen storage. Patent No. CN109027683A describes a hydrogen storage system and control method, the method adopts a catalytic bed mode to perform catalytic hydrogenation, the required catalyst amount is large, and most of the hydrogen storage catalysts are noble metal catalysts, and the use cost is high. For a trickle bed small test device, when the granular catalyst is used for catalytic hydrogenation, the hydrogen storage material flows down along the pipe wall, the contact area is small, and the hydrogen storage efficiency is seriously influenced.
Therefore, it is desirable to provide a system for storing liquid organic hydrogen, which can increase the contact area between the material and the catalyst and increase the reaction efficiency.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide a liquid organic hydrogen storage system and an intermittent feeding reaction device, wherein the intermittent feeding is carried out on a trickle bed by adopting a mode of controlling a hydrogen storage material by an electromagnetic valve, so that the contact area between the material and a catalyst is increased, and the reaction efficiency is improved.
In one aspect, the present invention discloses a liquid organic hydrogen storage device, comprising:
a feed system for introducing gas and hydrogen storage material;
the reaction system comprises an intermittent feeding reaction device, a hydrogen storage material hydrogenation device and a hydrogen storage material hydrogenation device, wherein the intermittent feeding reaction device is used for hydrogenating the hydrogen storage material to react;
and the separation system is used for separating and collecting the hydrogenated hydrogen storage material and the redundant hydrogen.
As a further improvement of the embodiment of the invention, the feeding system comprises a hydrogen tank, a storage tank, a preheating furnace and a quality meter buffer tank which are connected in sequence;
and an electromagnetic valve is arranged at the outlet end of the feeding system, and a digital electric contact pressure gauge is installed at the front end of the electromagnetic valve and used for controlling the maximum or minimum pressure value of the opening and closing of the electromagnetic valve, so that intermittent feeding is realized.
As a further improvement of the embodiment of the invention, a fan-shaped nozzle is welded at the upper end of the feeding hole of the intermittent feeding reaction device, and the fan-shaped nozzle is made of stainless steel materials and is used for realizing the atomization of the hydrogen storage materials.
As a further improvement of the embodiment of the invention, the reaction system comprises a high-temperature ceramic fiber reaction electric furnace capable of temperature programming, a fixed bed reaction tube, a pressure sensor and a thermocouple;
the gas phase and the liquid phase are mixed at the upper end of the reaction system and enter the upper end of the reaction area, when the liquid pressure reaches the set maximum value of the electromagnetic valve, the electromagnetic valve is opened, and the liquid is sprayed by the fan-shaped nozzle to enter a fixed bed reaction tube of the intermittent feeding reaction device in an atomized mode, so that the hydrogenation of the hydrogen storage material is realized.
As a further improvement of the embodiment of the present invention, the separation system includes a condenser, a gas-liquid separator, a collection tank; the hydrogenated liquid is condensed by a condenser and then is separated in a gas-liquid separator, the liquid enters a collecting tank, and the gas enters an emptying system.
As a further improvement of the embodiment of the invention, the preheating furnace is further provided with a filter for filtering solid impurities which may be present when the liquid hydrogen storage material enters the preheating furnace through the advection pump.
As a further improvement of the embodiment of the invention, the fixed bed reaction tube is filled with a noble metal catalyst for hydrogenation reaction, and the fixed bed reaction tube is internally provided with a temperature probe for detecting the temperature of the reaction system.
As a further improvement of the embodiment of the invention, the condenser is a coil type and is internally provided with a wire mesh filter.
In another aspect, the invention discloses a method for storing liquid organic hydrogen, comprising the steps of:
s1, before the reaction starts, detecting the pipeline by using a helium leak detector, and purging the whole pipeline by using nitrogen under the condition that the pipeline is not gas-tight so that other impurity gases do not exist in the pipeline;
s2, heating to 200 ℃, introducing hydrogen, setting the pressure range of an electromagnetic valve to be 6.1-7.1MPa after the hydrogen pressure reaches 6MPa, setting the flow rate of a hydrogen storage material to be 5ml/min by an advection pump, opening the electromagnetic valve and the advection pump for feeding, and entering a reaction system;
s3, automatically opening the electromagnetic valve after the electromagnetic valve receives the liquid pressure signal, and enabling the liquid to enter the reaction system in a spray form and the gas to react in the intermittent feeding reaction device;
s4, condensing and gas-liquid separating the hydrogenated material flowing out of the reaction system, and then feeding the hydrogenated material into a collection tank;
s5, sampling at the collection tank for component analysis testing by GC-MS.
As a further improvement of the embodiment of the present invention, the batch feed reaction apparatus is filled with a catalyst packing, and the method for filling the catalyst packing includes: the length of the fixed bed reaction tube is 1000mm, the width of the upper end is 300mm, and gamma-alumina pellets with the particle size of 1.5mm are filled in the fixed bed reaction tube; the middle size is 600mm, and the ruthenium/alumina catalyst and the alumina pellets with the spherical grain diameter of 1.5mm are filled in the catalyst, and the proportion is 2: 1, the size of the lower end is 100mm, and a ruthenium/alumina catalyst and alumina pellets with the spherical particle size of 1.5mm are filled in the reactor, wherein the ratio of the ruthenium/alumina catalyst to the alumina pellets is 1: 1.
as a further improvement of the embodiment of the invention, the electromagnetic valve is made of a high-temperature and high-pressure resistant material, and a polytetrafluoroethylene gasket is required to be used as a sealing gasket in the electromagnetic valve, so that the gasket is prevented from being corroded by a solvent.
The device disclosed by the invention adopts the electromagnetic valve to control the hydrogen storage material to perform intermittent feeding on the trickle bed, so that the contact area of the material and the catalyst is increased, and the reaction efficiency is improved.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the embodiments or the prior art descriptions will be briefly introduced below;
FIG. 1 is a schematic diagram of a liquid organic hydrogen storage device according to an embodiment of the present invention;
FIG. 2 is a schematic view of a batch feed reaction apparatus according to an embodiment of the present invention;
FIG. 3 is a graph showing the results of GC-MS tests on the hydrogenated product in example 1;
FIG. 4 is a graph showing the results of GC-MS measurement of the hydrogenated product in example 2.
The examples in the figures are represented as:
1-hydrogen tank, 2-material storage tank, 3-preheating furnace, 4-quality meter buffer tank, 5-electromagnetic valve, 6-fan nozzle, 7-reaction system, 8-condenser, 9-gas-liquid separator and 10-collecting tank.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings.
The embodiment of the invention discloses a liquid organic hydrogen storage device, which comprises:
a feed system for introducing gas and hydrogen storage material;
the reaction system comprises an intermittent feeding reaction device, a hydrogen storage material hydrogenation device and a hydrogen storage material hydrogenation device, wherein the intermittent feeding reaction device is used for hydrogenating the hydrogen storage material to react;
and the separation system is used for separating and collecting the hydrogenated hydrogen storage material and the redundant hydrogen.
The feeding system comprises a hydrogen tank 1, a storage tank 2, a preheating furnace 3 and a quality meter buffer tank 4 which are connected in sequence;
an electromagnetic valve 5 is arranged at the outlet end of the feeding system, and a digital electric contact pressure gauge is installed at the front end of the electromagnetic valve 5 and used for controlling the maximum or minimum pressure value of the opening and closing of the electromagnetic valve 5, so that intermittent feeding is realized.
Particularly, in the embodiment of the invention, a fan-shaped nozzle 6 is welded at the upper end of the feeding hole of the intermittent feeding reaction device, and the fan-shaped nozzle 6 is made of stainless steel materials and is used for realizing the atomization of the hydrogen storage materials.
In the embodiment of the invention, the reaction system 7 comprises a high-temperature ceramic fiber reaction electric furnace capable of temperature programming, a fixed bed reaction tube, a pressure sensor and a thermocouple;
the gas phase and the liquid phase are mixed and enter the upper end of the reaction area at the upper end of the reaction system, when the liquid pressure reaches the set maximum value of the electromagnetic valve 5, the electromagnetic valve 5 is opened, and the liquid is sprayed by the fan-shaped nozzle 6 to enter a fixed bed reaction tube of the intermittent feeding reaction device in an atomized mode, so that the hydrogenation of the hydrogen storage material is realized.
In the embodiment of the present invention, the separation system includes a condenser 8, a gas-liquid separator 9, a collection tank 10; the hydrogenated liquid is condensed by a condenser 8 and then separated in a gas-liquid separator, the liquid enters a collecting tank, and the gas enters an emptying system.
Further, the preheating furnace 3 is also provided with a filter for filtering solid impurities which may exist when the liquid hydrogen storage material enters the preheating furnace 3 through the advection pump.
Specifically, the inside of the fixed bed reaction tube is filled with a noble metal catalyst for hydrogenation reaction, and the inside is provided with a temperature probe for detecting the temperature of the reaction system.
In the present embodiment, the condenser 8 is a coil type, and a wire mesh filter is arranged in the condenser.
The embodiment of the invention also discloses a liquid organic hydrogen storage method, which comprises the following steps:
s1, before the reaction starts, detecting the pipeline by using a helium leak detector, and purging the whole pipeline by using nitrogen under the condition that the pipeline is not gas-tight so that other impurity gases do not exist in the pipeline;
s2, heating to 200 ℃, introducing hydrogen, setting the pressure range of an electromagnetic valve to be 6.1-7.1MPa after the hydrogen pressure reaches 6MPa, setting the flow rate of a hydrogen storage material to be 5ml/min by an advection pump, opening the electromagnetic valve and the advection pump for feeding, and entering a reaction system;
s3, automatically opening the electromagnetic valve after the electromagnetic valve receives the liquid pressure signal, and enabling the liquid to enter the reaction system in a spray form and the gas to react in the intermittent feeding reaction device;
s4, condensing and gas-liquid separating the hydrogenated material flowing out of the reaction system, and then feeding the hydrogenated material into a collection tank;
s5, sampling at the collection tank for component analysis testing by GC-MS.
Specifically, a batch feed reaction device is filled with a catalyst filler, and the filling method of the catalyst filler comprises the following steps: the length of the fixed bed reaction tube is 1000mm, the width of the upper end is 300mm, and gamma-alumina pellets with the particle size of 1.5mm are filled in the fixed bed reaction tube; the middle size is 600mm, and the ruthenium/alumina catalyst and the alumina pellets with the spherical grain diameter of 1.5mm are filled in the catalyst, and the proportion is 2: 1, the size of the lower end is 100mm, and a ruthenium/alumina catalyst and alumina pellets with the spherical particle size of 1.5mm are filled in the reactor, wherein the ratio of the ruthenium/alumina catalyst to the alumina pellets is 1: 1.
furthermore, the electromagnetic valve 5 is made of a high-temperature and high-pressure resistant material, and a polytetrafluoroethylene gasket is needed for a sealing gasket inside the electromagnetic valve 5, so that the gasket is prevented from being corroded by a solvent.
Example 1:
benzyl toluene is used as a hydrogen storage raw material:
step a: before the reaction starts, a helium leak detector is used for detecting the pipeline, and under the condition that the pipeline is ensured not to leak gas, nitrogen is used for purging the whole pipeline, so that other impurity gases do not exist in the pipeline;
step b: after the temperature is raised to 200 ℃, hydrogen is introduced. In the process of introducing hydrogen, the temperature is slightly reduced, and after the pressure of the hydrogen reaches 6MPa, the temperature is kept for a period of time to be stable. At the moment, the pressure range of the electromagnetic valve is set to be 6.1-7.1MPa, and the flow rate of the benzyltoluene is set to be 5ml/min by the advection pump. When the temperature returns to the preset temperature, the electromagnetic valve and the advective pump are opened for feeding;
step c: after the electromagnetic valve receives a liquid pressure signal, the valve is automatically opened, liquid enters a reaction system in a spray form to react with gas, and the temperature is obviously increased in the reaction process;
step d: the hydrogenated material flowing out of the reaction furnace enters a collecting tank after condensation and gas-liquid separation. Sampling at the collection tank tested for GC-MS and the results are shown in fig. 3 with 99.94% of the product being fully hydrogenated to 12H product.
Example 2:
dibenzyl toluene is used as a hydrogen storage raw material:
step a: before the reaction starts, a helium leak detector is used for detecting the pipeline, and under the condition that the pipeline is ensured not to leak gas, nitrogen is used for purging the whole pipeline, so that other impurity gases do not exist in the pipeline;
step b: after the temperature is raised to 200 ℃, hydrogen is introduced. In the process of introducing hydrogen, the temperature is slightly reduced, and after the pressure of the hydrogen reaches 7MPa, the temperature is kept for a period of time to be stable. At the moment, the pressure range of the electromagnetic valve is set to be 7.1-8.1MPa, and the flow rate of dibenzyl toluene is set to be 2ml/min by the advection pump. When the temperature returns to the preset temperature, the electromagnetic valve and the advective pump are opened for feeding;
step c: after the electromagnetic valve receives a liquid pressure signal, the valve is automatically opened, liquid enters a reaction system in a spray form to react with gas, and the temperature is obviously increased in the reaction process;
step d: the hydrogenated material flowing out of the reaction furnace enters a collecting tank after condensation and gas-liquid separation. Sampling at the collection tank tested for GC-MS and the results are shown in fig. 4 with 91.23% of the product being fully hydrogenated to 18H product.
In example 2, dibenzyltoluene had a higher viscosity than in example 1, and had to be diluted with cyclohexane before use.
The device disclosed by the invention adopts the electromagnetic valve to control the hydrogen storage material to perform intermittent feeding on the trickle bed, so that the contact area of the material and the catalyst is increased, and the reaction efficiency is improved.
It will be apparent to those skilled in the art that various changes and modifications can be made without departing from the inventive concept thereof, and these changes and modifications can be made without departing from the spirit and scope of the invention.
Claims (10)
1. A liquid organic hydrogen storage device, comprising:
a feed system for introducing gas and hydrogen storage material;
the reaction system comprises an intermittent feeding reaction device, a hydrogen storage material hydrogenation device and a hydrogen storage material hydrogenation device, wherein the intermittent feeding reaction device is used for hydrogenating the hydrogen storage material to react;
and the separation system is used for separating and collecting the hydrogenated hydrogen storage material and the redundant hydrogen.
2. The liquid organic hydrogen storage device according to claim 1, wherein the feeding system comprises a hydrogen tank, a storage tank, a preheating furnace, a quality meter buffer tank which are connected in sequence;
and an electromagnetic valve is arranged at the outlet end of the feeding system, and a digital electric contact pressure gauge is installed at the front end of the electromagnetic valve and used for controlling the maximum or minimum pressure value of the opening and closing of the electromagnetic valve, so that intermittent feeding is realized.
3. The liquid organic hydrogen storage device of claim 2, wherein a fan-shaped nozzle is welded to the upper end of the feed inlet of the batch-type feeding reaction device, and the fan-shaped nozzle is made of stainless steel and is used for atomizing the hydrogen storage material.
4. The liquid organic hydrogen storage device of claim 3, wherein the reaction system comprises a temperature programmable high temperature ceramic fiber reaction electric furnace and fixed bed reaction tube, a pressure sensor, a thermocouple;
the gas phase and the liquid phase are mixed at the upper end of the reaction system and enter the upper end of the reaction area, when the liquid pressure reaches the set maximum value of the electromagnetic valve, the electromagnetic valve is opened, and the liquid is sprayed by the fan-shaped nozzle to enter a fixed bed reaction tube of the intermittent feeding reaction device in an atomized mode, so that the hydrogenation of the hydrogen storage material is realized.
5. The liquid organic hydrogen storage device of claim 1, wherein the separation system comprises a condenser, a gas-liquid separator, a collection tank; the hydrogenated liquid is condensed by a condenser and then is separated in a gas-liquid separator, the liquid enters a collecting tank, and the gas enters an emptying system.
6. The liquid organic hydrogen storage device of claim 2, wherein the preheating furnace is further provided with a filter for filtering solid impurities that may be present when the liquid hydrogen storage material enters the preheating furnace via the advection pump.
7. The liquid organic hydrogen storage device according to claim 4, wherein the fixed bed reaction tube is filled with a noble metal catalyst for hydrogenation reaction and has a temperature probe therein for detecting the temperature of the reaction system.
8. The system for liquid organic hydrogen storage according to claim 5, wherein the condenser is a coil type with wire mesh filtration built in.
9. A method for storing liquid organic hydrogen, said method comprising the steps of:
s1, before the reaction starts, detecting the pipeline by using a helium leak detector, and purging the whole pipeline by using nitrogen under the condition that the pipeline is not gas-tight so that other impurity gases do not exist in the pipeline;
s2, heating to 200 ℃, introducing hydrogen, setting the pressure range of an electromagnetic valve to be 6.1-7.1MPa after the hydrogen pressure reaches 6MPa, setting the flow rate of a hydrogen storage material to be 5ml/min by an advection pump, opening the electromagnetic valve and the advection pump for feeding, and entering a reaction system;
s3, automatically opening the electromagnetic valve after the electromagnetic valve receives the liquid pressure signal, and enabling the liquid to enter the reaction system in a spray form and the gas to react in the intermittent feeding reaction device;
s4, condensing and gas-liquid separating the hydrogenated material flowing out of the reaction system, and then feeding the hydrogenated material into a collection tank;
s5, sampling at the collection tank for component analysis testing by GC-MS.
10. The method for storing liquid organic hydrogen according to claim 9, wherein the batch feed reactor is filled with a catalyst packing, and the method for filling the catalyst packing comprises: the length of the fixed bed reaction tube is 1000mm, the width of the upper end is 300mm, and gamma-alumina pellets with the particle size of 1.5mm are filled in the fixed bed reaction tube; the middle size is 600mm, and the ruthenium/alumina catalyst and the alumina pellets with the spherical grain diameter of 1.5mm are filled in the catalyst, and the proportion is 2: 1, the size of the lower end is 100mm, and a ruthenium/alumina catalyst and alumina pellets with the spherical particle size of 1.5mm are filled in the reactor, wherein the ratio of the ruthenium/alumina catalyst to the alumina pellets is 1: 1.
optionally, the electromagnetic valve needs to be made of high-temperature and high-pressure resistant materials, and a polytetrafluoroethylene gasket is needed for a sealing gasket inside the electromagnetic valve, so that the gasket is prevented from being corroded by a solvent.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114893721A (en) * | 2022-05-13 | 2022-08-12 | 北京瀚锐氢能科技有限公司 | Organic liquid hydrogen storage system based on intelligent automation |
| CN115138263A (en) * | 2022-07-27 | 2022-10-04 | 嘉兴联合化学有限公司 | Special organosilicon phenyl monomer preparation and separation purification device |
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| CN1565958A (en) * | 2003-06-10 | 2005-01-19 | 中国科学院大连化学物理研究所 | Catalyst for making hydrogen of hydrogenous inorganic compound aqueous solution and hydrogen making process |
| CN210595250U (en) * | 2019-06-14 | 2020-05-22 | 广东国能中林实业有限公司 | Hydrogenation system for liquid hydrogen storage carrier |
| CN212549471U (en) * | 2020-12-31 | 2021-02-19 | 苏州金宏气体股份有限公司 | Liquid organic hydrogen storage and release system |
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| CN1565958A (en) * | 2003-06-10 | 2005-01-19 | 中国科学院大连化学物理研究所 | Catalyst for making hydrogen of hydrogenous inorganic compound aqueous solution and hydrogen making process |
| CN210595250U (en) * | 2019-06-14 | 2020-05-22 | 广东国能中林实业有限公司 | Hydrogenation system for liquid hydrogen storage carrier |
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| CN114893721A (en) * | 2022-05-13 | 2022-08-12 | 北京瀚锐氢能科技有限公司 | Organic liquid hydrogen storage system based on intelligent automation |
| CN115138263A (en) * | 2022-07-27 | 2022-10-04 | 嘉兴联合化学有限公司 | Special organosilicon phenyl monomer preparation and separation purification device |
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